HRID1637704
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred solution of 5-cyanoindole (1.0 g, 7.0 mmol), K2CO3 (0.966 g, 7.0 mmol) in acetonitrile was added 3-bromomethylpropionate (1.17 g, 7.0 mmol). The mixture was stirred at reflux for 18 h under a nitrogen atmosphere, cooled, diluted with H2O, extracted with ethyl acetate, dried with Na2SO4, filtered and concentrated in vacuo to afford 1.59 g of product. 1H NMR (CD3OD) δppm 2.85 (t, 2H, J=6.6 Hz), 3.61 (s, 3H), 4.58 (t, 2H, J=6.6 Hz), 6.61 (s, 1H), 7.42, (m, 3H), 7.62 (d, 1H, J=8.4 Hz), 7.99 (s, 1H).
WORKUP
后处理
- temperatureat reflux for 18 h under a nitrogen atmosphere
- temperaturecooled
- extractionextracted with ethyl acetate
- dry with materialdried with Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo